CN113718363B - Water-jet composite non-woven fabric and preparation method thereof - Google Patents

Water-jet composite non-woven fabric and preparation method thereof Download PDF

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CN113718363B
CN113718363B CN202111036819.XA CN202111036819A CN113718363B CN 113718363 B CN113718363 B CN 113718363B CN 202111036819 A CN202111036819 A CN 202111036819A CN 113718363 B CN113718363 B CN 113718363B
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modified polypropylene
parts
filtering
washing
drying
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CN113718363A (en
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何福明
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Zhejiang Dale Nonwoven New Materials Co ltd
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Zhejiang Dale Nonwoven New Materials Co ltd
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    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/44Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
    • D01F6/46Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F255/00Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00
    • C08F255/02Macromolecular compounds obtained by polymerising monomers on to polymers of hydrocarbons as defined in group C08F10/00 on to polymers of olefins having two or three carbon atoms
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F8/00Chemical modification by after-treatment
    • C08F8/40Introducing phosphorus atoms or phosphorus-containing groups
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00General methods for the manufacture of artificial filaments or the like
    • D01F1/02Addition of substances to the spinning solution or to the melt
    • D01F1/10Other agents for modifying properties
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/44Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
    • D04H1/46Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
    • D04H1/492Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres by fluid jet
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/542Adhesive fibres
    • D04H1/544Olefin series
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
    • D04H1/54Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving
    • D04H1/56Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by welding together the fibres, e.g. by partially melting or dissolving in association with fibre formation, e.g. immediately following extrusion of staple fibres

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Mechanical Engineering (AREA)
  • Nonwoven Fabrics (AREA)

Abstract

The invention provides a spunlaced composite non-woven fabric and a preparation method thereof, and belongs to the technical field of spunlaced fabrics. The preparation method comprises the following steps: 100-150 parts of modified polypropylene, 10-15 parts of silane coupling agent and 2-5 parts of graphene oxide; the modified polypropylene has the structure shown below; wherein n=100-200. The composite spun-laced non-woven fabric has excellent antibacterial and antistatic effects, good mechanical properties, washing resistance and weather resistance, and firm fiber web, and the high-performance spun-laced non-woven fabric is obtained.

Description

Water-jet composite non-woven fabric and preparation method thereof
Technical Field
The invention relates to the technical field of spunlaced fabrics, in particular to a spunlaced composite non-woven fabric and a preparation method thereof.
Background
The non-woven fabric has the characteristics of ventilation, softness, light weight, no toxicity or irritation, rich colors, low price and the like. If polypropylene (PP) granules are used as raw materials, the polypropylene (PP) granules are produced by a continuous one-step method of high-temperature melting, spinning, lapping, hot-pressing coiling. The spun-laced non-woven fabric is one of non-woven fabrics, and is obtained by spraying high-pressure micro water flow onto one or more layers of fiber webs to enable the fibers to be intertwined with each other, so that the fiber webs are reinforced and have certain strength, and the obtained fabric is the spun-laced non-woven fabric.
In order to increase the strength of the nonwoven fabric without changing the performance of the nonwoven fabric, the mechanical performance and the bonding capability of the nonwoven fabric are improved by adopting a hydroentangling method, but the antistatic performance and the antibacterial performance of the hydroentangled nonwoven fabric are further improved, so that the composite hydroentangled nonwoven fabric is necessary to be proposed.
Patent CN109177353A discloses a compound water thorn non-woven fabrics, is three-layer composite structure, and upper and lower layers are water thorn non-woven fabrics layer, and the intermediate level is the enhancement layer, the enhancement layer of upper strata water thorn non-woven fabrics layer, intermediate level and the water thorn non-woven fabrics layer three of lower floor consolidate as an organic wholely, consolidate as an organic wholely through the water thorn, have improved the powerful poor problem of traditional water thorn non-woven fabrics, have improved the tensile strength of water thorn non-woven fabrics greatly. However, the spunlaced nonwoven fabric has high hardness and poor softness.
Patent CN113026201a discloses a composite nanofiber spunlaced nonwoven fabric, which is mainly prepared from PP fibers, nanocellulose fibers, carbon fibers and polyester fibers in proportion. Compared with the prior art, the water-jet nonwoven fabric has the advantages of good structural strength, tissue compactness, environmental protection and the like, but the preparation process of the water-jet nonwoven fabric is complex, and the industrial production is not easy.
Disclosure of Invention
The invention aims to provide a spunlaced composite non-woven fabric and a preparation method thereof, which have good antibacterial and antistatic properties and obviously improved mechanical properties.
The technical scheme of the invention is realized as follows:
the invention provides a spunlaced composite non-woven fabric which is prepared from the following raw materials: modified polypropylene, a silane coupling agent and graphene oxide;
the modified polypropylene has a structure shown in a formula I:
wherein n=100-200.
As a further improvement of the invention, the invention is prepared from the following raw materials in parts by weight: 100-150 parts of modified polypropylene, 10-15 parts of silane coupling agent and 2-5 parts of graphene oxide.
As a further improvement of the present invention, the modified polypropylene is prepared by the following method:
s1, mixing a 3-butene-1-amine monomer, polypropylene and an initiator, heating and melting, performing graft copolymerization reaction, filtering, washing with ethanol, and drying to obtain an intermediate, wherein the intermediate has a structure shown in a formula II:
s2, preparation of triphenyl phosphonium bromide: dissolving triphenylphosphine and 1, 2-dibromopropane in a first solvent, heating for reaction, filtering, washing with diethyl ether, and drying to obtain triphenylphosphine bromide, wherein the triphenylphosphine bromide has a structure shown in a formula III:
s3, preparing modified polypropylene: and (2) dissolving the triphenylphosphine bromide in the step (S2) in a second solvent, adding the intermediate in the step (S1), stirring for reaction under the protection of nitrogen, filtering, washing with ethanol, adding the mixture into hydrochloric acid solution, stirring for reaction, filtering, and drying to obtain the modified polypropylene.
As a further improvement of the present invention, the modified polypropylene is prepared by the following method:
s1, mixing 60-75 parts by weight of 3-butene-1-amine monomer, 50-60 parts by weight of polypropylene and 0.1-0.5 part by weight of initiator, heating to 180-220 ℃, reacting for 2-3 hours, filtering, washing with ethanol, and drying to obtain an intermediate;
s2, preparation of triphenyl phosphonium bromide: dissolving 25-27 parts by weight of triphenylphosphine and 21-22 parts by weight of 1, 2-dibromopropane in a first solvent, heating to 120-140 ℃ for reaction for 1-2h, filtering, washing with diethyl ether, and drying to obtain triphenylphosphine bromide;
s3, preparing modified polypropylene: dissolving 45-50 parts by weight of the triphenylphosphine bromide in the step S2 into a second solvent, adding 10-15 parts by weight of the intermediate in the step S1, heating to 40-60 ℃ under the protection of nitrogen, stirring for reaction, filtering, washing with ethanol, adding into 1-2mol/L hydrochloric acid solution, stirring for reaction for 0.5-1h, filtering, and drying to obtain the modified polypropylene.
As a further improvement of the invention, the initiator is selected from one or more of azodiisobutyronitrile, azodiisoheptonitrile, tert-butyl hydroperoxide, benzoyl peroxide, lauroyl peroxide, di-tert-butyl peroxide, tert-butyl peroxybenzoate, dicumyl peroxide, cyclohexanone peroxide, tert-butyl peroxyvalerate, methyl ethyl ketone peroxide, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, sodium persulfate, potassium persulfate and ammonium persulfate.
As a further improvement of the present invention, the first solvent is at least one selected from the group consisting of xylene, toluene, benzene, ethylbenzene, propylbenzene, diethylbenzene; the second solvent is at least one selected from dichloromethane, chloroform, tetrahydrofuran, acetonitrile, toluene and benzene.
As a further improvement of the invention, the silane coupling agent is a silane coupling agent with amino group and is selected from one or more of gamma-aminopropyl trimethoxysilane, gamma-aminopropyl triethoxysilane, N-beta (aminoethyl) -gamma-aminopropyl trimethoxysilane, N-beta (aminoethyl) -gamma-aminopropyl triethoxysilane, N-beta (aminoethyl) -gamma-aminopropyl methyldimethoxy silane, N-beta (aminoethyl) -gamma-aminopropyl methyldiethoxy silane and diethylenetriaminopropyl trimethoxysilane.
As a further improvement of the invention, the silane coupling agent is a compound mixture of gamma-aminopropyl trimethoxysilane and N-beta (aminoethyl) -gamma-aminopropyl methyl diethoxy silane, and the mass ratio is (2-5): 1.
the invention further provides a preparation method of the spunlaced composite non-woven fabric, which comprises the following steps:
(1) Adding modified polypropylene into ethanol water solution containing silane coupling agent, heating to 80-90 ℃, reacting for 1-2h, adding graphene oxide, continuing to react for 0.5-1h, adjusting pH to 8-10 with ammonia water, continuing to react for 3-4h, filtering, washing with ethanol, and obtaining SiO 2 Modified polypropylene;
(2) SiO is made of 2 Adding modified polypropylene into a screw injection molding machine, heating, melting and spinning, and stretching under the action of hot air to obtain SiO 2 Modified polypropylene fiber;
(3) SiO is made of 2 Drawing the modified polypropylene fiber by a drawing airflow, blowing the fiber to a roller, collecting the fiber on the roller, and bonding the fiber into cloth by self heat;
(4) Collecting the melt-blown non-woven fabric after being formed into a net on a roller, and coiling the net into a coil by a coiling mechanism;
(5) And (3) drafting the coiled cloth, loading the coiled cloth into a flat net hydroentangling machine, carrying out hydroentangling reinforcement, and drying after hydroentangling to obtain the hydroentangled composite non-woven fabric.
As a further improvement of the invention, the pressure of the water jet is 1.8-2.5MPa.
The invention has the following beneficial effects: the invention prepares modified polypropylene, after polypropylene and 3-butene-1-amine monomer are polymerized and modified, triphenyl phosphonium bromide is further connected, and hydrochloric acid is adopted for protonation, so that the modified polypropylene with quaternary ammonium salt and phosphonium salt sites is prepared, and the modified polypropylene has obvious antibacterial and antistatic effects, and the quaternary phosphonium salt and the quaternary ammonium salt have the advantages of high antibacterial efficiency, broad spectrum, wide pH application range, good chemical stability and the like, and firstly, the surface of bacterial cells with negative charges is adsorbed on the quaternary ammonium salt sites, then invades into cell walls, is further combined with cell membranes and causes cell membrane rupture; furthermore, the structure is also a cationic antistatic structure, the lipophilic group faces the inside of polypropylene, the hydrophilic group is arranged towards the atmosphere side, and the hydrophilic group absorbs moisture in the atmosphere to form a continuous and uniform conductive molecular layer with orientation characteristics on the surface of the product, so that the aggregation of static electricity is reduced, and therefore, the structure is also a long-acting water-resistant antistatic raw material, and the antistatic performance of the prepared spun-laced non-woven fabric is improved.
In the preparation of the composite spunlaced nonwoven fabric, modified polypropylene is further modified and coupled by a silane coupling agent with amino, and the silane part of the silane coupling agent is hydrolyzed to generate SiO under alkaline condition 2 The fiber is fixed on the surface of modified polypropylene, the mechanical property of the polypropylene material is improved, and after the fiber is further reinforced by hydroentanglement, the fiber in the fiber web is displaced, penetrated, entangled and cohesive to form countless flexible entangled points, so that the fiber web is reinforced, and the high-performance hydroentangled non-woven fabric is obtained.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a synthetic route diagram of the modified polypropylene of the present invention.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Preparation example 1 modified Polypropylene
The synthetic route is shown in figure 1, and is prepared by the following method:
s1, mixing 60g of 3-butene-1-amine monomer, 50g of polypropylene and 0.1g of lauroyl peroxide, heating to 180 ℃, reacting for 2 hours, filtering, washing with ethanol, and drying to obtain an intermediate;
s2, preparation of triphenyl phosphonium bromide: dissolving 25g of triphenylphosphine and 21g of 1, 2-dibromopropane in 100mL of toluene, heating to 120 ℃ for reaction for 1h, filtering, washing with diethyl ether, and drying to obtain triphenylphosphine bromide;
s3, preparing modified polypropylene: 45g of the triphenylphosphine bromide in the step S2 is dissolved in 100mL of chloroform, 10g of the intermediate in the step S1 is added, the mixture is heated to 40 ℃ under the protection of nitrogen, the mixture is stirred and reacted for 3 hours, the mixture is filtered, washed by ethanol, added into 1mol/L hydrochloric acid solution, stirred and reacted for 1 hour, filtered and dried, and the modified polypropylene is obtained.
PREPARATION EXAMPLE 2 modified Polypropylene
The synthetic route is shown in figure 1, and is prepared by the following method:
s1, mixing 75g of 3-butene-1-amine monomer, 60g of polypropylene and 0.5g of tert-butyl peroxypivalate, heating to 220 ℃, reacting for 3 hours, filtering, washing with ethanol, and drying to obtain an intermediate;
s2, preparation of triphenyl phosphonium bromide: 27g of triphenylphosphine and 22g of 1, 2-dibromopropane are dissolved in 100mL of toluene, heated to 140 ℃ for reaction for 2 hours, filtered, washed by diethyl ether and dried to obtain triphenylphosphine bromide;
s3, preparing modified polypropylene: 50g of the triphenylphosphine bromide in the step S2 is dissolved in 100mL of chloroform, 15 parts by weight of the intermediate in the step S1 is added, the mixture is heated to 60 ℃ under the protection of nitrogen, the mixture is stirred and reacted for 3 hours, the mixture is filtered, washed by ethanol, added into 1mol/L hydrochloric acid solution, stirred and reacted for 1 hour, filtered and dried, and the modified polypropylene is obtained.
PREPARATION EXAMPLE 3 modified Polypropylene
The synthetic route is shown in figure 1, and is prepared by the following method:
s1, mixing 65g of 3-butene-1-amine monomer, 55g of polypropylene and 0.3g of azodiisoheptonitrile, heating to 200 ℃, reacting for 2.5h, filtering, washing with ethanol, and drying to obtain an intermediate;
s2, preparation of triphenyl phosphonium bromide: 26g of triphenylphosphine and 21.5g of 1, 2-dibromopropane are dissolved in 100mL of dimethylbenzene, heated to 130 ℃ for reaction for 1.5h, filtered, washed by diethyl ether and dried to obtain triphenylphosphine bromide;
s3, preparing modified polypropylene: 47g of the triphenylphosphine bromide in the step S2 is dissolved in 100mL of chloroform, 12g of the intermediate in the step S1 is added, the mixture is heated to 50 ℃ under the protection of nitrogen, the mixture is stirred and reacted for 3 hours, the mixture is filtered, washed by ethanol, added into 1mol/L hydrochloric acid solution, stirred and reacted for 1 hour, filtered and dried, and the modified polypropylene is obtained.
Comparative preparation example 1
In comparison with preparation 3, no modification with triphenylphosphine bromide was carried out, and the other conditions were unchanged.
The preparation method comprises the following steps:
s1, mixing 65g of 3-butene-1-amine monomer, 55g of polypropylene and 0.3g of azodiisoheptonitrile, heating to 200 ℃, reacting for 2.5h, filtering, washing with ethanol, and drying to obtain an intermediate;
s2, preparing modified polypropylene: 59g of the intermediate in the step S1 is added into 1mol/L hydrochloric acid solution, stirred and reacted for 1h, filtered and dried to obtain the modified polypropylene.
Example 1 Water-entangled composite nonwoven fabric
The preparation method comprises the following steps:
(1) 100g of modified polypropylene prepared in preparation example 1 is added into 500mL of ethanol aqueous solution containing 10g of silane coupling agent, heated to 85 ℃, added with 2g of graphene oxide after 2h of reaction, continuously reacted for 1h, adjusted to pH 9 by ammonia water, continuously reacted for 4h, filtered and washed by ethanol to obtain SiO 2 Modified polypropylene;
the silane coupling agent is a compound mixture of gamma-aminopropyl trimethoxysilane and N-beta (aminoethyl) -gamma-aminopropyl methyl diethoxy silane, and the mass ratio is 2:1.
(2) SiO is made of 2 Adding modified polypropylene into a screw injection molding machine, heating, melting and spinning, and stretching under the action of hot air to obtain SiO 2 Modified polypropylene fiber;
(3) SiO is made of 2 Drawing the modified polypropylene fiber by a drawing airflow, blowing the fiber to a roller, collecting the fiber on the roller, and bonding the fiber into cloth by self heat;
(4) Collecting the melt-blown non-woven fabric after being formed into a net on a roller, and coiling the net into a coil by a coiling mechanism;
(5) And (3) placing the coiled cloth into a flat net hydroentangling machine after drafting, carrying out hydroentangling reinforcement, carrying out hydroentangling at a hydroentangling head pressure of 2MPa, and drying to obtain the hydroentangling composite non-woven fabric.
Example 2
Compared with example 1, the raw materials and the proportions thereof are different, and other conditions are not changed.
The raw materials comprise: 150g of modified polypropylene prepared in preparation example 2, 15g of silane coupling agent and 5g of graphene oxide. The silane coupling agent is a compound mixture of gamma-aminopropyl trimethoxysilane and N-beta (aminoethyl) -gamma-aminopropyl methyl diethoxy silane, and the mass ratio is 5:1.
example 3
Compared with example 1, the raw materials and the proportions thereof are different, and other conditions are not changed.
The raw materials comprise: 125g of modified polypropylene prepared in preparation example 3, 12g of silane coupling agent and 3g of graphene oxide. The silane coupling agent is a compound mixture of gamma-aminopropyl trimethoxysilane and N-beta (aminoethyl) -gamma-aminopropyl methyl diethoxy silane, and the mass ratio is 3:1.
example 4
In comparison with example 3, the silane coupling agent was gamma-aminopropyl trimethoxysilane, and the other conditions were not changed.
Example 5
In comparison with example 3, the silane coupling agent was N-beta (aminoethyl) -gamma-aminopropyl methyldiethoxysilane, the other conditions not being changed.
Comparative example 1
In comparison with example 3, the modified polypropylene was replaced by that prepared in comparative preparation 1, and the other conditions were not changed.
Comparative example 2
In comparison with example 3, the modified polypropylene was replaced by a normal polypropylene, and the other conditions were not changed.
Comparative example 3
In comparison with example 3, no silane coupling agent was added, and the other conditions were not changed.
Comparative example 4
In comparison with example 3, no graphene oxide was added, and the other conditions were not changed.
Test example 1 antibacterial and anti-mite Performance test
The spunlaced composite nonwoven fabrics prepared in examples 1-5 and comparative examples 1-4 were tested by the oscillation method (GB/T20944.3-2008). The results are shown in Table 1.
TABLE 1
Group of Coli antibacterial efficiency (%) Staphylococcus aureus antibacterial rate (%)
Example 1 96.7 97.2
Example 2 97.1 98.0
Example 3 98.9 99.2
Example 4 94.2 95.4
Example 5 93.7 96.2
Comparative example 1 83.5 82.0
Comparative example 2 65.2 60.1
Comparative example 3 92.2 93.4
Comparative example 4 88.5 89.2
The spunlaced composite non-woven fabrics prepared in examples 1-5 and comparative examples 1-4 were subjected to mite-proof test, and the test indexes are according to national standard GBT24253-2009, and the results are shown in Table 2.
TABLE 2
Group of Mite-proof rate (%)
Example 1 89
Example 2 92
Example 3 95
Example 4 90
Example 5 91
Comparative example 1 75
Comparative example 2 56
Comparative example 3 89
Comparative example 4 84
As shown in the table above, the spun-laced composite non-woven fabric prepared by the invention has good antibacterial and anti-mite properties.
Test example 2 Performance test
The spun-laced composite non-woven fabrics prepared in examples 1-5 and comparative examples 1-4 were subjected to performance test, and tested according to the technical requirement method of GB/T21295-2014 clothing physical and chemical properties, and the results are shown in Table 3.
TABLE 3 Table 3
Group of Breaking strength (N) Bursting strength (N) Tearing strength (N) Wearing weight (mg)
Example 1 990 740 48 0.3
Example 2 997 752 49 0.3
Example 3 1005 760 50 0.2
Example 4 920 702 42 0.5
Example 5 902 698 43 0.6
Comparative example 1 980 730 47 0.4
Comparative example 2 940 720 46 0.4
Comparative example 3 840 670 39 0.9
Comparative example 4 880 690 40 0.7
As can be seen from the above table, the spun-laced composite non-woven fabric prepared by the invention has good mechanical properties, tear resistance and wear resistance.
Test example 3
The spunlaced composite nonwoven fabrics prepared in examples 1-5 and comparative examples 1-4 were subjected to surface resistance test, and the results are shown in Table 4, according to AATCC 76-2019, textile surface resistance test method.
TABLE 4 Table 4
As shown in the table above, the spun-laced composite non-woven fabric prepared by the invention has lower surface resistance and excellent antistatic performance.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.

Claims (6)

1. The spunlaced composite non-woven fabric is characterized by being prepared from the following raw materials in parts by weight: 100-150 parts of modified polypropylene, 10-15 parts of silane coupling agent and 2-5 parts of graphene oxide; the silane coupling agent is a compound mixture of A174 and A172, and the mass ratio is (2-5): 1, a step of;
the modified polypropylene has a structure shown in a formula I:
wherein n=100-200;
the modified polypropylene is prepared by the following method:
s1, mixing a 3-butene-1-amine monomer, polypropylene and an initiator, heating and melting, performing graft copolymerization reaction, filtering, washing with ethanol, and drying to obtain an intermediate, wherein the intermediate has a structure shown in a formula II:
s2, preparation of triphenyl phosphonium bromide: dissolving triphenylphosphine and 1, 2-dibromopropane in a first solvent, heating for reaction, filtering, washing with diethyl ether, and drying to obtain triphenylphosphine bromide, wherein the triphenylphosphine bromide has a structure shown in a formula III:
s3, preparing modified polypropylene: and (2) dissolving the triphenylphosphine bromide in the step (S2) in a second solvent, adding the intermediate in the step (S1), stirring for reaction under the protection of nitrogen, filtering, washing with ethanol, adding the mixture into hydrochloric acid solution, stirring for reaction, filtering, and drying to obtain the modified polypropylene.
2. The spunlaced composite nonwoven fabric of claim 1, wherein the modified polypropylene is prepared by the following method:
s1, mixing 60-75 parts by weight of 3-butene-1-amine monomer, 50-60 parts by weight of polypropylene and 0.1-0.5 part by weight of initiator, heating to 180-220 ℃, reacting for 2-3 hours, filtering, washing with ethanol, and drying to obtain an intermediate;
s2, preparation of triphenyl phosphonium bromide: dissolving 25-27 parts by weight of triphenylphosphine and 21-22 parts by weight of 1, 2-dibromopropane in a first solvent, heating to 120-140 ℃ for reaction for 1-2h, filtering, washing with diethyl ether, and drying to obtain triphenylphosphine bromide;
s3, preparing modified polypropylene: dissolving 45-50 parts by weight of the triphenylphosphine bromide in the step S2 into a second solvent, adding 10-15 parts by weight of the intermediate in the step S1, heating to 40-60 ℃ under the protection of nitrogen, stirring for reaction, filtering, washing with ethanol, adding into 1-2mol/L hydrochloric acid solution, stirring for reaction for 0.5-1h, filtering, and drying to obtain the modified polypropylene.
3. The spunlaced composite nonwoven fabric according to claim 1 or 2, wherein the initiator is selected from one or more of azobisisobutyronitrile, azobisisoheptonitrile, tert-butyl hydroperoxide, benzoyl peroxide, lauroyl peroxide, di-tert-butyl peroxide, tert-butyl peroxybenzoate, dicumyl peroxide, cyclohexanone peroxide, tert-butyl peroxyvalerate, methyl ethyl ketone peroxide, diisopropyl peroxydicarbonate, dicyclohexyl peroxydicarbonate, sodium persulfate, potassium persulfate and ammonium persulfate.
4. The spun-laced composite nonwoven fabric of claim 1 or 2, wherein the first solvent is selected from at least one of xylene, toluene, benzene, ethylbenzene, propylbenzene, diethylbenzene; the second solvent is at least one selected from dichloromethane, chloroform, tetrahydrofuran, acetonitrile, toluene and benzene.
5. A method of making a hydroentangled composite nonwoven fabric as defined in any one of claims 1-4, comprising the steps of:
(1) Adding modified polypropylene into ethanol water solution containing silane coupling agent, heating to 80-90 ℃, reacting for 1-2h, adding graphene oxide, continuing to react for 0.5-1h, adjusting pH to 8-10 with ammonia water, continuing to react for 3-4h, filtering, washing with ethanol, and obtaining SiO 2 Modified polypropylene;
(2) SiO is made of 2 Adding modified polypropylene into a screw injection molding machine, heating, melting and spinning, and stretching under the action of hot air to obtain SiO 2 Modified poly (ethylene-propylene) copolymerPropylene fibers;
(3) SiO is made of 2 Drawing the modified polypropylene fiber by a drawing airflow, blowing the fiber to a roller, collecting the fiber on the roller, and bonding the fiber into cloth by self heat;
(4) Collecting the melt-blown non-woven fabric after being formed into a net on a roller, and coiling the net into a coil by a coiling mechanism;
(5) And (3) drafting the coiled cloth, loading the coiled cloth into a flat net hydroentangling machine, carrying out hydroentangling reinforcement, and drying after hydroentangling to obtain the hydroentangled composite non-woven fabric.
6. The method according to claim 5, wherein the pressure of the hydroentangling head is 1.8-2.5MPa.
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